CN103613957A - Preparation method of novel zirconium-aluminum-coated titanium dioxide - Google Patents

Preparation method of novel zirconium-aluminum-coated titanium dioxide Download PDF

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CN103613957A
CN103613957A CN201310557368.3A CN201310557368A CN103613957A CN 103613957 A CN103613957 A CN 103613957A CN 201310557368 A CN201310557368 A CN 201310557368A CN 103613957 A CN103613957 A CN 103613957A
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slurry
tio
solution
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60min
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苏振宇
魏旭芳
徐敬丽
张磊
张兵兵
李茂恩
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LUOHE XINGMAO TITANIUM INDUSTRY Co Ltd
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LUOHE XINGMAO TITANIUM INDUSTRY Co Ltd
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Abstract

The invention relates to a preparation method of novel zirconium-aluminum-coated titanium dioxide. The method is simple in process, easy to operate, efficient and simple in production process, short in coating period and beneficial to lowering production energy consumption. Moreover, titanium dioxide pigment prepared by the method has higher gloss, weather resistance, whiteness and other excellent pigment performances.

Description

A kind of preparation method of novel zirconium-aluminium coated titanium white powder
Technical field
The invention belongs to rutile titanium dioxide surface-treated technological method, be specifically related to the titanium dioxide process of a kind of high brightness, high whiteness, high glossiness.
Background technology
Rutile titanium dioxide, because of its high refractive index and excellent pigment performance, is considered to best in the world white pigment, is widely used in the industries such as coating, plastics, papermaking, ink.Titanium dioxide has high photocatalytic activity, and not surface treated titanium dioxide exists some lattice imperfections, makes to exist on its particle surface many photoactivation points.In being applied in the fields such as coating, plastics, in atmosphere, with the organic composition can catalyzed degradation under ultraviolet irradiation contacting with it, the phenomenon such as cause base-material xanthochromia, efflorescence, even chap, peel off, has a strong impact on work-ing life and the performance of product.
In order to improve the use properties of titanium dioxide, must carry out surface treatment modification to titanium dioxide.In recent years, people use aluminum oxide (Al conventionally 2o 3), silicon-dioxide (SiO 2) etc. oxide compound titanium dioxide surface is coated, sial coating can effectively prevent titanium dioxide photochemical activity, and the two easy coprecipitated surface at TiO 2 particles.Domestic and international high-grade titanium dioxide generally adopts zirconium white (ZrO at present 2), the oxide compound such as aluminum oxide carries out surface treatment, ZrO 2good coated treatment agent as titanium dioxide surface, can promote Al 2o 3etc. outer treatment agent and matrix TiO 2adhere to.Zirconia-alumina coating can significantly be sheltered the lip-deep optical active group of titanium dioxide lattice, reduces the photochemical activity of titanium dioxide, and does not affect TiO 2brightness and color, contribute to improve the durable and dispersing property of titanium white powder pigment.Therefore, Zirconia-alumina coating TiO 2product has higher glossiness, weathering resistance and whiteness.Yet the research of domestic Zr-Al coating is less, and its complex technical process, complex operation, production cycle are longer, and capsulation condition is controlled also more harsh.
Summary of the invention
The present invention is directed to titanium dioxide process for treating surface present situation, a kind of new coating method is provided, the method technique is simple, easy handling, and production process is efficiently simple and direct, and the coated cycle is short, is conducive to the reduction of production energy consumption.And the TiO 2 pigment of preparing by the method has higher glossiness, weathering resistance, whiteness and other excellent pigment performance.
Technical scheme of the present invention is
A preparation method for novel zirconium-aluminium coated titanium white powder, is characterized in that comprising the following steps.
Step 1, first, by the elementary grinding work in-process of a certain amount of rutile titanium dioxide, its particle diameter is 0.2-0.3 μ m, then adopts Sodium hexametaphosphate 99 alkaline aqueous solution to carry out dispersion treatment and makes slurry.The concentration of described sodium hexametaphosphate solution is with P 2o 5count 40g/L, wherein P 2o 5account for TiO in elementary grinding work in-process 20.06% of quality meter.
Step 2, is warmed up to 50-90 ℃ by dispersion disposed slurry, and keeps this temperature.
Step 3 by the slurry in step 2, evenly adds water-soluble zirconium sulfate solution in 20-60min, and wherein the add-on of water-soluble zirconium sulfate solution is with ZrO 2meter is TiO in slurry 2the 0.4%-1.0% of amount, regulates slurry PH5.0-6.5, slaking 10-60min with the NaOH aqueous solution., temperature remains on 50-90 ℃.
Step 4 adds the sodium metaaluminate aqueous solution in 20-60min, and wherein the add-on of aluminum salt solution is with Al 2o 3meter is slurry TiO 2the 1.0%-3.0% of amount, slaking 10-60min, temperature remains on 50-90 ℃.
Step 5 adds aluminum sulfate aqueous solution in 30-90min, and wherein the add-on of aluminum salt solution is with Al 2o 3meter is TiO in slurry 2the 1.5%-4.0% of amount, slaking 10-60min, temperature remains on 50-90 ℃.
Step 6, adds the NaOH aqueous solution, regulates slurry PH7.0-8.0, slaking 1-3h, and temperature remains on 50-90 ℃.
Step 7, carries out filtration washing to filtrate resistivity with 40-70 ℃ of de-salted water and is less than 100 μ s/m, is dried, pulverization process, makes TiO 2 pigment sample.
Described, zirconium sulfate strength of solution is with ZrO 2count 80-110g/L; Sodium aluminate solution concentration is with Al 2o 3count 100-160g/L; Alum liquor concentration is with Al 2o 3count 80-110g/L.
Described, TiO 2middle rutile crystal type content is more than 98%.
Beneficial effect:
The TiO that the present invention adopts 2in first product, rutile crystal type content, more than 98%, guarantees the pigment performances such as basic opacifying power of product; By to TiO 2the adjustment of first product slurry PH, effectively controls the front pulp particle of coating and exists with precursor, guarantees coated ZrO 2evenly, this layer of fine and close hydrated aluminum oxide film is conducive to improve TiO 2 pigment optical property and dispersing property.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
1, the slurry of Rutile type Titanium Dioxide first product being made to 300g/L, adds sodium hexametaphosphate solution, wherein P 2o 5account for TiO in first product 20.06% of quality meter, the concentration of sodium hexametaphosphate solution is with P 2o 5count 40g/L, the NaOH solution that is 20% by concentration regulates slurry PH9.5-10.5, dispersed with stirring 40min.
2, the slurry after disperseing is warmed up to 60 ℃, and makes whole coating process maintain this temperature.
3, in 40min, evenly add with ZrO 2meter accounts for TiO in first product 2quality is 0.5% zirconium sulfate solution, and the concentration of zirconium sulfate solution is with ZrO 2count 100g/L, dispersed with stirring 20min.
4, in 30min, with 10%NaOH solution, slowly regulate slurry PH to 5.0-6.5, slaking 60min.
5, at 20min, evenly add with Al 2o 3account for TiO in first product 2quality is counted 1.5% sodium aluminate solution, and sodium aluminate solution concentration is with Al 2o 3count 120g/L, slaking 20min.
6, in 40min, evenly add with Al 2o 3meter accounts for TiO in first product 2quality is 2% alum liquor, and alum liquor concentration is with Al 2o 3count 100g/L, slaking 60min.
7, in 30min, evenly add 10% the NaOH aqueous solution, regulate slurry PH7.2-7.6, insulation slaking 120min.
8, with 50 ℃ of de-salted waters, carry out filtration washing to filtrate resistivity and be less than 100 μ s/m, dry 24h at 120 ℃, and use high Shearing pulverizer pulverization process, obtain TiO 2 pigment.
Embodiment 2
1, the slurry of Rutile type Titanium Dioxide first product being made to 300g/L, adds sodium hexametaphosphate solution, wherein P 2o 5account for TiO in first product 20.06% of quality meter, the concentration of sodium hexametaphosphate solution is with P 2o 5count 40g/L, the NaOH solution that is 20% by concentration regulates slurry PH9.5-10.5, dispersed with stirring 40min.
2, the slurry after disperseing is warmed up to respectively to 70 ℃, and makes whole coating process maintain this temperature.
3, following operation is with the 3-8 step operation in embodiment 1.
Embodiment 3
1, the slurry of Rutile type Titanium Dioxide first product being made to 300g/L, adds sodium hexametaphosphate solution, wherein P 2o 5account for TiO in first product 20.06% of quality meter, the concentration of sodium hexametaphosphate solution is with P 2o 5count 40g/L, the NaOH solution that is 20% by concentration regulates slurry PH9.5-10.5, dispersed with stirring 40min.
2, the slurry after disperseing is warmed up to respectively to 80 ℃, and makes whole coating process maintain this temperature.
3, following operation is with the 3-8 step operation in embodiment 1.
Embodiment 4
1, the slurry of Rutile type Titanium Dioxide first product being made to 300g/L, adds sodium hexametaphosphate solution, wherein P 2o 5for TiO in first product 20.1% of quality, the concentration of sodium hexametaphosphate solution is with P 2o 5count 40g/L, the NaOH solution that is 20% by concentration regulates slurry PH9.5-10.5, dispersed with stirring 40min.
2, the slurry after disperseing is warmed up to respectively to 60 ℃, and makes whole coating process maintain this temperature.
3, in 40min, evenly add with ZrO 2count TiO in first product 2quality is 0.5% zirconium sulfate solution, and the concentration of zirconium sulfate solution is with ZrO 2count 100g/L, dispersed with stirring 20min.
4, in 30min, with 10%NaOH solution, slowly regulate slurry PH to 5.0-6.5, slaking 60min.
5, at 20min, evenly add with Al 2o 3account for TiO in first product 2quality is counted 1.5% sodium aluminate solution, and sodium aluminate solution concentration is with Al 2o 3count 120g/L, slaking 20min.
6, in 40min, evenly add with Al 2o 3account for TiO in first product 2quality is counted 2.5% alum liquor, and alum liquor concentration is with Al 2o 3count 100g/L, slaking 60min.
7, following operation is with the 7-8 step operation in embodiment 1.
Embodiment 5
1, the slurry of Rutile type Titanium Dioxide first product being made to 300g/L, adds sodium hexametaphosphate solution, wherein P 2o 5for TiO in first product 20.1% of quality, the concentration of sodium hexametaphosphate solution is with P 2o 5count 40g/L, the NaOH solution that is 20% by concentration regulates slurry PH9.5-10.5, dispersed with stirring 40min.
2, the slurry after disperseing is warmed up to respectively to 60 ℃, and makes whole coating process maintain this temperature.
3, in 40min, evenly add with ZrO 2count TiO in first product 2quality is 0.6% zirconium sulfate solution, and the concentration of zirconium sulfate solution is with ZrO 2count 100g/L, dispersed with stirring 20min.
4, following operation is with the 4-8 step operation in embodiment 1.
Provide the detected result of embodiment of the present invention zirconium-aluminium coating below
Figure BSA0000097409330000041
Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.

Claims (3)

1. a preparation method for novel zirconium-aluminium coated titanium white powder, is characterized in that comprising the following steps:
Step 1, first, by the elementary grinding work in-process of a certain amount of rutile titanium dioxide, its particle diameter is 0.2-0.3 μ m, then adopts Sodium hexametaphosphate 99 alkaline aqueous solution to carry out dispersion treatment and makes slurry; The concentration of described sodium hexametaphosphate solution is with P 2o 5count 40g/L, wherein P 2o 5account for TiO in elementary grinding work in-process 20.06% of quality meter;
Step 2, is warmed up to 50-90 ℃ by dispersion disposed slurry, and keeps this temperature;
Step 3 by the slurry in step 2, evenly adds water-soluble zirconium sulfate solution in 20-60min, and wherein the add-on of water-soluble zirconium sulfate solution is with ZrO 2meter is TiO in slurry 2the 0.4%-1.0% of amount, regulates slurry PH5.0-6.5 with the NaOH aqueous solution, slaking 10-60min, and temperature remains on 50-90 ℃;
Step 4 adds the sodium metaaluminate aqueous solution in 20-60min, and wherein the add-on of aluminum salt solution is with Al 2o 3meter is slurry TiO 2the 1.0%-3.0% of amount, slaking 10-60min, temperature remains on 50-90 ℃;
Step 5 adds aluminum sulfate aqueous solution in 30-90min, and wherein the add-on of aluminum salt solution is with Al 2o 3meter is TiO in slurry 2the 1.5%-4.0% of amount, slaking 10-60min, temperature remains on 50-90 ℃;
Step 6, adds the NaOH aqueous solution, regulates slurry PH7.0-8.0, slaking 1-3h, and temperature remains on 50-90 ℃;
Step 7, carries out filtration washing to filtrate resistivity with 40-70 ℃ of de-salted water and is less than 100 μ s/m, is dried, pulverization process, makes TiO 2 pigment sample.
2. the preparation method of a kind of novel zirconium-aluminium coated titanium white powder according to claim 1, described in it is characterized in that, zirconium sulfate strength of solution is with ZrO 2count 80-110g/L; Sodium aluminate solution concentration is with Al 2o 3count 100-160g/L; Alum liquor concentration is with Al 2o 3count 80-110g/L.
3. the preparation method of a kind of novel zirconium-aluminium coated titanium white powder according to claim 1, described in it is characterized in that, TiO 2middle rutile crystal type content is more than 98%.
CN201310557368.3A 2013-11-12 2013-11-12 Preparation method of novel zirconium-aluminum-coated titanium dioxide Pending CN103613957A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104031432A (en) * 2014-06-27 2014-09-10 安徽金星钛白(集团)有限公司 Novel surface treatment method of phosphorus, aluminum and zirconium-coated TiO2
CN105860591A (en) * 2016-05-05 2016-08-17 中钛集团洛阳市裕星化工有限公司 Preparation method of novel zirconium-aluminum coated titanium dioxide
CN108864770A (en) * 2018-09-05 2018-11-23 襄阳龙蟒钛业有限公司 A kind of preparation method of low oil absorption ferric titanium dioxide
CN108997790A (en) * 2018-09-05 2018-12-14 襄阳龙蟒钛业有限公司 A kind of high glaze titanium white production method
CN109054453A (en) * 2018-09-05 2018-12-21 襄阳龙蟒钛业有限公司 A kind of low oil absorption ferric titanium dioxide
CN112759948A (en) * 2020-12-30 2021-05-07 攀枝花东方钛业有限公司 Special titanium dioxide for road sign paint and preparation method thereof
CN113563739A (en) * 2021-07-29 2021-10-29 安徽金星钛白(集团)有限公司 Preparation method of composite coated titanium dioxide for bactericidal coating
CN114539815A (en) * 2022-03-01 2022-05-27 昆明冶金研究院有限公司 High-covering high-dispersity modified micro silicon powder and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101463195A (en) * 2007-12-21 2009-06-24 衡阳天友化工有限公司 Red schorl type titanium dioxide coating method and preparation of used reagent

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101463195A (en) * 2007-12-21 2009-06-24 衡阳天友化工有限公司 Red schorl type titanium dioxide coating method and preparation of used reagent

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104031432A (en) * 2014-06-27 2014-09-10 安徽金星钛白(集团)有限公司 Novel surface treatment method of phosphorus, aluminum and zirconium-coated TiO2
CN105860591A (en) * 2016-05-05 2016-08-17 中钛集团洛阳市裕星化工有限公司 Preparation method of novel zirconium-aluminum coated titanium dioxide
CN105860591B (en) * 2016-05-05 2018-05-18 焦作市裕盛钛业有限公司 A kind of preparation method of novel zirconium-aluminum-ctitanium titanium dioxide
CN108864770A (en) * 2018-09-05 2018-11-23 襄阳龙蟒钛业有限公司 A kind of preparation method of low oil absorption ferric titanium dioxide
CN108997790A (en) * 2018-09-05 2018-12-14 襄阳龙蟒钛业有限公司 A kind of high glaze titanium white production method
CN109054453A (en) * 2018-09-05 2018-12-21 襄阳龙蟒钛业有限公司 A kind of low oil absorption ferric titanium dioxide
CN112759948A (en) * 2020-12-30 2021-05-07 攀枝花东方钛业有限公司 Special titanium dioxide for road sign paint and preparation method thereof
CN112759948B (en) * 2020-12-30 2022-05-10 攀枝花东方钛业有限公司 Special titanium dioxide for road sign paint and preparation method thereof
CN113563739A (en) * 2021-07-29 2021-10-29 安徽金星钛白(集团)有限公司 Preparation method of composite coated titanium dioxide for bactericidal coating
CN114539815A (en) * 2022-03-01 2022-05-27 昆明冶金研究院有限公司 High-covering high-dispersity modified micro silicon powder and preparation method thereof

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Application publication date: 20140305